CN107402252A - High temperature refractory mineral laser BrF5Method oxygen isotope composition analysis system and method - Google Patents
High temperature refractory mineral laser BrF5Method oxygen isotope composition analysis system and method Download PDFInfo
- Publication number
- CN107402252A CN107402252A CN201710656902.4A CN201710656902A CN107402252A CN 107402252 A CN107402252 A CN 107402252A CN 201710656902 A CN201710656902 A CN 201710656902A CN 107402252 A CN107402252 A CN 107402252A
- Authority
- CN
- China
- Prior art keywords
- metal
- 4inch
- trap
- valves
- cold
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 84
- 239000011707 mineral Substances 0.000 title claims abstract description 84
- 238000004458 analytical method Methods 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 62
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000001301 oxygen Substances 0.000 title claims abstract description 60
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 60
- 239000000203 mixture Substances 0.000 title claims abstract description 38
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 59
- 229910014271 BrF5 Inorganic materials 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000746 purification Methods 0.000 claims abstract description 27
- 238000005259 measurement Methods 0.000 claims abstract description 19
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 15
- 239000002699 waste material Substances 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 6
- 238000007872 degassing Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims description 691
- 229910052751 metal Inorganic materials 0.000 claims description 691
- 229910001220 stainless steel Inorganic materials 0.000 claims description 99
- 239000010935 stainless steel Substances 0.000 claims description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 76
- 150000001649 bromium compounds Chemical class 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 39
- 229910052757 nitrogen Inorganic materials 0.000 claims description 38
- 239000000047 product Substances 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 15
- 239000010931 gold Substances 0.000 claims description 15
- 229910052737 gold Inorganic materials 0.000 claims description 15
- 239000000376 reactant Substances 0.000 claims description 15
- -1 KBr metals Chemical class 0.000 claims description 12
- 230000008014 freezing Effects 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
- ADGTVSBGYUIMDS-UHFFFAOYSA-N FBr(C1=CC=CC=C1)(F)(F)(F)F Chemical compound FBr(C1=CC=CC=C1)(F)(F)(F)F ADGTVSBGYUIMDS-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003384 imaging method Methods 0.000 claims description 11
- 150000002739 metals Chemical class 0.000 claims description 11
- 239000002808 molecular sieve Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 6
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 5
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052794 bromium Inorganic materials 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 238000003556 assay Methods 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 239000003517 fume Substances 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000009897 systematic effect Effects 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- XHVUVQAANZKEKF-UHFFFAOYSA-N bromine pentafluoride Chemical compound FBr(F)(F)(F)F XHVUVQAANZKEKF-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 5
- 230000000155 isotopic effect Effects 0.000 abstract description 2
- 239000004519 grease Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000010450 olivine Substances 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical group FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 description 1
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910001423 beryllium ion Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to oxidiferous mineral isotopics to determine field, specifically discloses a kind of high temperature refractory mineral laser BrF5Method oxygen isotope composition analysis system and method, the one end of the reagent purification system of the system respectively with example reaction/separate/purification system, vacuum system connects, example reaction/separation/purification system other end is connected with one end of collection of products/measurement system, and the other end of collection of products/measurement system is connected with vacuum system；This method is as follows：High temperature refractory mineral samplers are analysed to load in analysis system；To the baking of a whole set of analysis system, vacuumize degassing；To the pre- fluorination treatment of high temperature refractory mineral samplers in sample laser cell；High temperature refractory mineral samplers in sample laser cell are carried out with fluorination reaction-O isotopes extraction；O2Purifying, collection and mass spectroscopy；Waste collection processing.The present invention improves high temperature refractory mineral oxygen isotope analysis measuring accuracy and analysis testing efficiency.
Description
Technical field
The invention belongs to oxidiferous mineral isotopics to determine field, and in particular to high temperature refractory mineral laser-BrF5Method
Oxygen isotope composition analysis system and method.
Background technology
Oxygen isotope is to study metallogenic material and the important means in BIFhosted gold deposit source, migration and evolution, to illustrate mineral deposit
Mineralizing genesis provides theoretical foundation.Fully extraction is that completion high temperature is difficult with converting the oxygen in mineral and it being purified, collected
Molten mineral (high temperature refractory mineral are usually formed temperature mostly more than 800 DEG C, reach as high as more than 2000 DEG C) oxygen isotope group
Into the premise of analysis.
It is basic both at home and abroad to be carried using conventional brominated bromide method in high temperature refractory mineral oxygen isotope analysis method
Analysis is taken, but this method has some drawback：1) sample size needed for experimental analysis is larger, at least needs 20mg sample, causes
Its spatial resolution is relatively low, will be unable to analyze for rare sample；2) the sample preparation cycle is grown, and causes analysis efficiency low
Under；3) because chemical time is grown, high to static system vacuum requirement, the polytetrafluoroethylene gasket that reactor uses exists
It is difficult to ensure that system vacuum, easily causes the oxygen in air and enter system and the same position of sample generation under high and low temperature alternate environment
Element exchanges, and separately because needing to carry out reaction overnight, very big potential safety hazard be present；4) the nickel reactant pipe used in is carrying out several high temperature difficulties
Easily contaminated and not easy cleaning, has a strong impact on sample analysis test result after molten sample analysis；5) held using external heat mode
The generation of nickel fluoride in reactor is easily caused, influences the measure of sample oxygen isotope composition.
In terms of test object, conventional method is that the oxygen for reacting generation is converted into CO under the high temperature conditions with graphite2
Carry out mass-spectrometer measurement.Because carbon has12C、13Two kinds of isotopes of C participate in calculating, it is necessary to be corrected to measurement result, convert simultaneously
Process easily causes O isotope fractionations；Conversion system needs to introduce glass pipeline, and wherein glass piston need to periodically smear vacuum grease
To ensure piston seal performance and rotate flexibility, smearing makes system be exposed to air during vacuum grease, the oxygen in air
Gas and water vapour pollutes into system, while vacuum sealing grease easily causes cross pollution because oxygen-containing.
The content of the invention
It is an object of the invention to provide a kind of new high temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system
System and method, solution high temperature refractory mineral sample consumption in oxygen isotope analysis is big, spatial resolution is low, oxygen extraction is endless
Entirely, conversion process easily causes the problems such as OXYGEN ISOTOPE FRACTIONATION, improves analysis measuring accuracy and analysis testing efficiency.
Realize the technical scheme of the object of the invention：A kind of high temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis
System, the system include reagent purification system, example reaction/separation/purification system, collection of products/measurement system and vacuum system
System；The one end of reagent purification system respectively with example reaction/separate/purification system, vacuum system connects, and example reaction/separation/
The purification system other end is connected with one end of collection of products/measurement system, the other end and the vacuum system of collection of products/measurement system
System connection.
Described reagent purification system includes rotary-vane pump, the first metal cold-trap, the storage of the first brominated bromide
Tank, pressure vacuum gauge, 1/2inch stainless steel pipes, the second brominated bromide holding vessel, tri pentafluorophenyl bromine holding vessel, the second gold medal
Belong to cold-trap, the top of 1/2inch stainless steel pipes is provided with pressure vacuum gauge, the side upper part of 1/2inch stainless steel pipes
It is not connected with the first brominated bromide holding vessel top exit, the first metal cold-trap entrance, the outlet of the first metal cold-trap and rotary vane type
Oil-sealed rotary pump inlet end connects；One side bottom of 1/2inch stainless steel pipes respectively with the second brominated bromide holding vessel, the 3rd
Brominated bromide holding vessel top exit connects, and another upper lateral part of 1/2inch stainless steel pipes and the second metal cold-trap entrance connect
Connect.
The 5th 1/4inch metal valves are provided between the top of described 1/2inch stainless steel pipes and pressure vacuum gauge.
The 4th 1/4inch metal valves are provided between described 1/2inch stainless steel pipes and the first brominated bromide holding vessel
Door, is provided with the 3rd 1/4inch metal valves, the first metal is cold between 1/2inch stainless steel pipes and the first metal cold-trap entrance
Trap exports is provided with the 2nd 1/4inch metal valves, the first metal cold-trap exit between rotary-vane pump inlet end
It is additionally provided with the first 1/4inch metal valve in parallel with the 2nd 1/4inch metal valves.
The 12nd is provided between described 1/2inch stainless steel pipes bottom and tri pentafluorophenyl bromine holding vessel top exit
1/4inch metal valves, the 11st 1/4inch metal valves, the 12nd 1/4inch metal valves, the 11st 1/4inch metals
The tenth 1/4inch metal valves, the 9th 1/4inch metal valves are provided between valve and the second brominated bromide holding vessel top exit
Door, the 8th 1/4inch being all connected with both is provided between the tenth 1/4inch metal valves and the 9th 1/4inch metal valves
Metal valve.
One middle side part of described 1/2inch stainless steel pipes is also connected with the 7th 1/4inch metal valves one end, and the 7th
The 1/4inch metal valves other end is connected with the 6th 1/4inch metal valves 1.
The 13rd is provided between the opposite side of described 1/2inch stainless steel pipes and the second metal cold-trap entrance
4inch metal valves connect, and the second metal cold-trap exit is provided with the first spherical bellows metal valve, the first spherical bellows
Metal valve is connected with vacuum system.
Described example reaction/separation/purification system includes the 3rd metal cold-trap, CO2Infrared laser, imaging system
System, sample laser cell, the 4th metal cold-trap, fifth metal cold-trap, KBr metals hot trap and the 6th metal cold-trap, the 3rd metal are cold
Trap entrance is connected with the 13rd 1/4inch metal valves of reagent purification system, the outlet of the 3rd metal cold-trap and sample laser cell
One end connection, the other end of sample laser cell is connected with one end of the 4th metal cold-trap, the other end of the 4th metal cold-trap and
One end connection of fifth metal cold-trap, the other end of fifth metal cold-trap are connected with one end of KBr metal hot traps, KBr metal fevers
The other end of trap is connected with one end of the 6th metal cold-trap, and the other end and the collection of products/measurement system of the 6th metal cold-trap connect
Connect；CO is provided with above sample laser cell2Infrared laser, CO2Infrared laser is provided with imaging system.
The 14th 1/4inch metal valves are provided between the 3rd described metal cold-trap entrance and 1/2inch stainless steel pipes
Door, the 15th 1/4inch metal valves, sample laser cell and the 4th are provided between the outlet of the 3rd metal cold-trap and sample laser cell
The second spherical bellows metal valve is provided between metal cold-trap, the 3rd is provided between the 4th metal cold-trap and fifth metal cold-trap
Spherical bellows metal valve, the 4th spherical bellows metal valve is provided between fifth metal cold-trap and KBr metal hot traps,
The 5th spherical bellows metal valve is provided between KBr metals hot trap and the 6th metal cold-trap, the 6th metal cold-trap is received with product
The 6th spherical bellows metal valve is provided between collection/measurement system.
Described collection of products/measurement system includes electric capacity vacuum meter, the 7th spherical bellows metal valve, the 8th spherical
Bellows metal valve, 1/2inch stainless steels collecting pipe, turbomolecular pump, isotope mass spectrometer, the 7th spherical bellows metal
One end of valve is connected by the 6th spherical bellows metal valve of pipeline and example reaction/separate/purification system, and electric capacity is true
Sky meter is connected with the 6th spherical bellows metal valve, the 7th spherical bellows metal valve respectively；7th spherical bellows gold
Belong to valve the other end respectively with the 8th spherical bellows metal valve, 1/2inch stainless steels collecting pipe and isotope mass spectrometry
Instrument connects.
Described vacuum system includes ion gauge and the turbomolecular pump using rotary vane mechanical pump as prime, turbine point
Sub- pump is connected with the first spherical bellows metal valve of reagent purification system, ion gauge respectively with turbomolecular pump,
One spherical bellows metal valve connection.
Described analysis system also includes waste treatment system, waste treatment system include the first 1/4inch metal valves,
2nd 1/4inch metal valves, rotary-vane pump, the first metal cold-trap, the 3rd 1/4inch metal valves, the 4th 1/
4inch metal valves, the first brominated bromide holding vessel, the 5th 1/4inch metal valves, 1/2inch stainless steel pipes, the 6th 1/
4inch metal valves, the 7th 1/4inch metal valves, the 14th 1/4inch metal valves, the 3rd metal cold-trap and the 15th
1/4inch metal valves, the first 1/4inch metal valves one end are connected with the outlet of the first metal cold-trap, the 2nd 1/4inch gold
One end of category valve is connected with the outlet of the first 1/4inch metal valves, the first metal cold-trap, the 2nd 1/4inch metal valves
The other end be connected with rotary-vane pump inlet end；The entrance and the 3rd 1/4inch metal valves of first metal cold-trap
One end connection, the other end of the 3rd 1/4inch metal valves is connected with 1/2inch stainless steel pipes；4th 1/4inch metals
One end of valve is connected with the first brominated bromide holding vessel, and the other ends of the 4th 1/4inch metal valves is respectively with the 3rd 1/
4inch metal valves, the connection of 1/2inch stainless steel pipes；The other end and 1/2inch of 5th 1/4inch metal valves are stainless
Steel conduit connects；One end of 7th 1/4inch metal valves is connected with 1/2inch stainless steel pipes, the 7th 1/4inch metal valves
The other end of door is connected with one end of the 6th 1/4inch metal valves；One end and 1/ of 14th 1/4inch metal valves
2inch stainless steel pipes are connected, and the other end of the 14th 1/4inch metal valves is connected with the entrance of the 3rd metal cold-trap, the
The outlet of three metal cold-traps is connected with one end of the 15th 1/4inch metal valves.
It is a kind of using high temperature refractory mineral laser-BrF described above5Method oxygen isotope composition analysis system carries out high temperature
Refractory mineral laser-BrF5The method of method oxygen isotope composition analysis, this method specifically comprise the following steps：
Step 1, it is analysed in high temperature refractory mineral samplers loading analysis system；
Step 2, a whole set of analysis system is toasted, vacuumizes degassing；
Step 3, to the pre- fluorination treatment of high temperature refractory mineral samplers in sample laser cell；
Step 4, the high temperature refractory mineral samplers in sample laser cell are carried out with fluorination reaction-O isotopes extraction；
Step 5, O2Purifying, collection and mass spectroscopy；
Step 6, waste collection processing.
Described step 1 comprises the following steps that：By CO2Infrared laser and imaging system from sample laser cell just
Top is removed, all valves in closing in the analysis system, opens sample laser cell, the high temperature refractory mineral sample being analysed to
Product load in clean sample disc and made a record, and the sample disc for filling high temperature refractory mineral samplers to be analyzed is placed on into sample
In product laser cell, close and tighten sample laser cell, complete dress sample operation.
Described step 2 comprises the following steps that：Open heating charged, the carry out heated baking to the analysis system；
The liquid nitrogen cup on the first metal cold-trap overcoat, the 15th 1/4inch metal valves and the 14th 1/4inch metal valves are opened,
First the partial air in sample laser cell is diffused in 1/2inch stainless steel tube main pipelines；Close the 15th 1/4inch metals
Valve, the 3rd 1/4inch metal valves and the 2nd 1/4inch metal valves are opened, 1/ is taken out by rotary-vane pump
Low vacuum in 2inch stainless steel pipes, close the 14th 1/4inch metal valves and the 3rd 1/4inch metal valves.Slowly beat
The 15th 1/4inch metal valves are opened, the air in sample laser cell is diffused into 1/2inch stainless steel pipes and led to by several times
Cross rotary-vane pump and take out low vacuum, it is final to open the 15th 1/4inch metal valves, the 14th 1/4inch gold completely
Belong to valve, the tenth 1/4inch metal valves and the 12nd 1/4inch metal valves；Open the 3rd 1/4inch metal valves and
In two 1/4inch metal valve sample drawing laser cells after sample low vacuum 20min, the 3rd 1/4inch metal valves are closed；
Liquid nitrogen cup on two metal cold-trap overcoats, open the first spherical bellows metal valve, the 3rd spherical bellows metal valve, the 4th
Spherical bellows metal valve, the 5th spherical bellows metal valve, the 6th spherical bellows metal valve, the 7th spherical ripple
Pipe metal valve and the 8th spherical bellows metal valve, turbomolecular pump is connected to continue to vacuumize after system pumping high vacuum
30min, pass through ion gauge monitoring system vacuum.
System heated baking temperature in described step 2 is 250 DEG C；Turbomolecular pump is system pumping high vacuum to vacuum
Spend for 10-6Pa。
Described step 3 comprises the following steps that：Heating charged is closed, treats that the analysis system is recovered to room temperature, the
Liquid nitrogen cup on three metal cold-traps and the first brominated bromide holding vessel overcoat；Close the tenth 1/4inch metal valves, the 12nd
4inch metal valves, the 14th 1/4inch metal valves, the 15th 1/4inch metal valves and the 13rd 1/4inch metals
Valve, after opening the 11st 1/4inch metal valves above tri pentafluorophenyl bromine holding vessel, the slow semi-open 12nd
4inch metal valves, the BrF diffused to by pressure vacuum gauge control in 1/2inch stainless steel tube main pipelines5Reagent pressure,
Close the 12nd 1/4inch metal valves；Open after the 14th 1/4inch metal valves in 1/2inch stainless steel tube main pipelines
BrF5It is chilled in the 3rd metal cold-trap, closes the 14th 1/4inch metal valves, remove the liquid nitrogen outside the 3rd metal cold-trap
Cup, the 3rd metal cold-trap naturally to thaw are recovered to room temperature；The 15th 1/4inch metal valves are opened, by BrF5Diffusion of reagents
After keeping 2min in sample laser cell, the 14th 1/4inch metal valves, the 4th 1/4inch metal valves are opened successively, will
Remaining BrF5Reagent is chilled in the first brominated bromide holding vessel, opens the 3rd 1/4inch metal valves and the 2nd 1/4inch gold
Belong to valve, it is impossible to freeze the Residual reactants got off after the freezing of the first metal cold-trap, taken out by rotary-vane pump
Walk, the 4th 1/4inch metal valves closed on the first brominated bromide holding vessel.
The BrF that pressure vacuum gauge control is diffused in 1/2inch stainless steel tube main pipelines in described step 35Reagent pressure
Strong is 0.02MPa.
By above-mentioned steps 3 method in triplicate, fluorination treatment is carried out to sample in sample laser cell and inwall, last
Secondary BrF5Reagent retains 2h in sample laser cell, and removing high temperature refractory mineral samplers and sample laser cell inwall adsorb completely
Steam.
Described step 4 comprises the following steps that：High temperature refractory mineral samplers in sample laser cell are completed at pre- fluorination
After reason, 10 are reached to the analysis system pumping high vacuum-6Continue to take out 30min after Pa, close all valves；Outside the 3rd metal cold-trap
Liquid nitrogen cup is put, opens the 11st 1/4inch metal valves on tri pentafluorophenyl bromine holding vessel, opens the 5th 1/4inch gold
After belonging to valve, slow semi-open 12nd 1/4inch metal valves, the BrF repeatedly purified is passed through by pressure vacuum gauge control5
Reagent 0.01MPa is diffused in 1/2inch stainless steel tube main pipelines, closes the 11st 1/4inch metal valves and the 12nd
4inch metal valves；The 14th 1/4inch metal valves are opened by the BrF in pipeline5Reagent is refrigerated to the 3rd metal cold-trap
It is interior, close the 14th 1/4inch metal valves；Remove the liquid nitrogen cup outside the 3rd metal cold-trap to recover to room temperature, open the 15th
1/4inch metal valves are by BrF5In diffusion of reagents to sample laser cell, the 15th 1/4inch metal valves are closed；By CO2It is red
Outer laser is transferred to directly over sample laser cell, by imaging system position to high temperature refractory mineral samplers to be analyzed just on
Side, by CO2The laser beam of infrared laser is guided to the sample well for filling high temperature refractory mineral samplers to be analyzed, adjusts CO2It is infrared
The laser facula size and energy of lasers of laser, high temperature refractory mineral samplers to be analyzed are heated, high temperature refractory ore deposit
Thing sample at high temperature with BrF5Reagent carries out reaction and discharges oxygen, completes the extraction of sample O isotopes.
Described step 5 comprises the following steps that：The 4th metal cold-trap, fifth metal cold-trap, the 6th metal cold-trap and
Liquid nitrogen cup on 1/2inch stainless steel collecting pipe overcoats, the second spherical bellows metal valve is slowly opened, will be anti-in laser cell
Answer thing and remnants BrF5Reagent is chilled in the 4th metal cold-trap；The 3rd spherical bellows metal valve is opened after 10min, is led to
Fifth metal cold-trap is crossed to reactant and remnants BrF5Reagent freezes again；The 4th spherical bellows metal valve is opened after 5min
Door, by KBr metals hot trap to reactant and remnants BrF5Reagent further absorbs；The 5th spherical bellows is opened after 5min
Metal valve, the O by the 6th metal cold-trap to generation2Further freezing purifying；The 6th spherical bellows gold is opened after 5min
Belong to valve, reaction generation O is monitored by electric capacity vacuum meter2Pressure；Open the 7th spherical bellows metal valve, O2It is collected
To fillingIn the 1/2inch stainless steel collecting pipes of molecular sieve, O is monitored by electric capacity vacuum meter2Situation about being collected, treats O2Quilt
The 7th spherical bellows metal valve is closed after collecting completely；The liquid nitrogen outside 1/2inch stainless steel collecting pipes is removed, is recovered to room
O after temperature2It is released, the O that will be discharged2Introduce isotope mass spectrometer and carry out isotope assay.
It is filled with 1/2inch stainless steel collecting pipes in described step 5Molecular sieve.
Described step 6 comprises the following steps that：In the first metal cold-trap, the first brominated bromide holding vessel and the 3rd metal
Liquid nitrogen cup on cold-trap overcoat, the 6th spherical bellows metal valve is closed, open the 3rd 1/4inch metal valves, the 14th
4inch metal valves, the 15th 1/4inch metal valves, the second spherical bellows metal valve, the 3rd spherical bellows metal
Valve, the 4th spherical bellows metal valve and the 5th spherical bellows metal valve, by BrF remaining in system5Reagent and
Reactant is entered by the first metal cold-trap, the 3rd metal cold-trap, the 4th metal cold-trap, fifth metal cold-trap, the 6th metal cold-trap
After row fully freezing；The 2nd 1/4inch metal valves of slow opening are taken away by rotary-vane pump can not be cold by liquid nitrogen
The foreign gas of jelly, close the 3rd 1/4inch metal valves, the 4th spherical bellows metal valve and the 5th spherical bellows gold
Belong to valve；The liquid nitrogen cup outside the 3rd metal cold-trap, the 4th metal cold-trap, fifth metal cold-trap and the 6th metal cold-trap is removed, is treated
Cold-trap recovers to room temperature, opens the 4th 1/4inch metal valves by the first metal cold-trap, the 3rd metal cold-trap, the 4th metal
The remaining BrF of freezing in cold-trap, fifth metal cold-trap, the 6th metal cold-trap5Reagent and reaction product are refrigerated to the one or five fluorination
In bromine holding vessel；The 4th 1/4inch metal valves are closed, open the 3rd 1/4inch metal valves, the 4th spherical bellows metal
Valve and the 5th spherical bellows metal valve, low vacuum is further taken out to systematic pipeline by rotary-vane pump, will
Remaining impurity is frozen in the first metal cold-trap in the analysis system；All valves are closed, are removed outside the first metal cold-trap
Liquid nitrogen cup, successively open the 6th 1/4inch metal valves, the 7th 1/4inch metal valves, the 3rd 1/4inch metal valves and
First 1/4inch metal valves, the Litter of residual is downloaded in the lime bucket in fume hood with Ar fates, completed at waste
Put.
The advantageous effects of the present invention are：The present invention uses CO2Infrared laser is as high temperature refractory mineral samplers
Heater, high temperature caused by laser can make within a very short time high temperature refractory mineral be fluorinated and oxygen is discharged completely
Come, avoid in conventional method due to the reaction time is long cause sample-preparing system permanent vacuum reduce caused by oxygen isotope
Fractionation problem, while can be realized the advantages that laser facula is small, energy is concentrated, light beam homogenizes degree high, power continuously adjustabe pair
Micro-example (being less than 1mg) is analyzed, and can also realize that micro-zone in situ (125~6000um) is analyzed to particular sample；System gas
Road uses 316 stainless steel metal pipeline designs, avoids in conventional method because using vacuum sealing grease institute using glass pipeline
Oxydant is brought to disturb；Metal pipe line and laser cell outer wall wind heating tape, are easy to carry out vacuum bakeout degassing to system,
Reduce the influence of oxygen and steam to sample test in air；UsingMolecular sieve generates in the case where liquid nitrogen fully freezes to reaction
Oxygen directly collect carry out mass-spectrometer measurement, avoid measurement result need to be corrected by the introducing of graphite in conventional method
Problem, the defects of overcoming glass piston periodically to smear vacuum grease fat and system is exposed air, while avoid because use contains
Cross pollution caused by oxygen vacuum sealing grease；It is the turbomolecular pump of prime as system Gao Zhen to use rotary vane mechanical pump
Empty pump group, it is ensured that total system reaches higher vacuum, and further reduce oxygen-containing gas in air influences to caused by experimentation；
System is carried out by the way of spherical Bellows valve is combined using poly- trifluoro-ethylene valve and controlled, avoids valve because connecing for a long time
The problem of touching brominated bromide reagent and causing valve body corrosion sealing property to decline；The design pair combined using multiple cold-traps with hot trap
The oxygen of reaction release is purified step by step, thoroughly except the accessory substance of dereaction generation and remnants brominated bromide reagent, protection
Collection system and isotope mass spectrometer；Brominated bromide reagent holding vessel is made using Kel F material, passes through naked eyes
Observation can determine reagent storage and use state in holding vessel, and design three brominated bromide reagent holding vessels and be respectively used to deposit
Store up primary purity, high grade and the remaining brominated bromide of reaction；Whole system is after baking, sample are fluorinated remove steam in advance, and 25
Minute can complete heating, reaction, purifying and the isotope analysis operation of a sample, and analysis efficiency is greatly improved, is divided
It is higher to analyse result preci-sion and accuracy, error range is better than ± 0.2 ‰.
Brief description of the drawings
Fig. 1 is a kind of high temperature refractory mineral laser-BrF provided by the present invention5Method oxygen isotope composition analysis system is shown
It is intended to.
In figure：1 is the first 1/4inch metal valves, and 2 be the 2nd 1/4inch metal valves, and 3 be rotary vane type mechanical vacuum
Pump, 4 be the first metal cold-trap, and 5 be the 3rd 1/4inch metal valves, and 6 be the 4th 1/4inch metal valves, and 7 be the one or five fluorine
Change bromine holding vessel, 8 be pressure vacuum gauge, and 9 be the 5th 1/4inch metal valves, and 10 be 1/2inch stainless steel pipes, and 11 be the
Six 1/4inch metal valves, 12 be the 7th 1/4inch metal valves, and 13 be the 8th 1/4inch metal valves, and 14 be the 9th 1/
4inch metal valves, 15 be the second brominated bromide holding vessel, and 16 be the tenth 1/4inch metal valves, and 17 be the 11st
4inch metal valves, 18 be tri pentafluorophenyl bromine holding vessel, and 19 be the 12nd 1/4inch metal valves, and 20 be the 13rd
4inch metal valves, 21 be the second metal cold-trap, and 22 be the first spherical bellows metal valve, and 23 be the 14th 1/4inch gold
Belong to valve, 24 be the 3rd metal cold-trap, and 25 be the 15th 1/4inch metal valves, and 26 be CO2Infrared laser, 27 be imaging
Observing system, 28 be sample laser cell, and 29 be the second spherical bellows metal valve, and 30 be the 4th metal cold-trap, and 31 be the 3rd
Spherical bellows metal valve, 32 be fifth metal cold-trap, and 33 be the 4th spherical bellows metal valve, and 34 be KBr metal fevers
Trap, 35 be the 5th spherical bellows metal valve, and 36 be the 6th metal cold-trap, and 37 be the 6th spherical bellows metal valve, 38
It is the 7th spherical bellows metal valve for electric capacity vacuum meter, 39,40 be the 8th spherical bellows metal valve, and 41 be filling
The 1/2inch stainless steel collecting pipes of molecular sieve, 42 be ion gauge, and 43 be turbomolecular pump, and 44 be isotope mass spectrometer.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
A kind of as shown in figure 1, high temperature refractory mineral laser-BrF5The system of method oxygen isotope composition analysis, the system bag
Include reagent purification system, example reaction/separation/purification system, collection of products/measurement system, vacuum system and waste processing system
System.
Reagent purification system includes the first 1/4inch metal valves 1, the 2nd 1/4inch metal valves 2, rotary vane type machinery
Vavuum pump 3, the first metal cold-trap 4, the 3rd 1/4inch metal valves 5, the 4th 1/4inch metal valves 6, the first brominated bromide
Holding vessel 7, pressure vacuum gauge 8, the 5th 1/4inch metal valves 9,1/2inch stainless steel pipes 10, the 6th 1/4inch metals
Valve 11, the 7th 1/4inch metal valves 12, the 8th 1/4inch metal valves 13, the 9th 1/4inch metal valves 14, second
Brominated bromide holding vessel 15, the tenth 1/4inch metal valves 16, the 11st 1/4inch metal valves 17, the storage of tri pentafluorophenyl bromine
Deposit tank 18, the 12nd 1/4inch metal valves 19, the 13rd 1/4inch metal valves 20, the second metal cold-trap 21 and the first ball
Shape bellows metal valve 22.The outlet that the one end of first 1/4inch metal valves 1 passes through lateral line and the first metal cold-trap 4
Connection, one end of the 2nd 1/4inch metal valves 2 are connected by threeway with the lateral line, the 2nd 1/4inch metal valves 2
The other end be connected by pipeline with the inlet end of rotary-vane pump 3.The entrance of first metal cold-trap 4 passes through pipeline and
One end connection of three 1/4inch metal valves 5, the other end of the 3rd 1/4inch metal valves 5 pass through 1/4inch stainless steel tubes
Line is weldingly connected with 1/2inch stainless steel pipes 10；One end of 4th 1/4inch metal valves 6 passes through 1/4inch stainless steel tubes
Line is connected with the top exit of the first brominated bromide holding vessel 7, and the other end of the 4th 1/4inch metal valves 6 is distinguished by threeway
It is connected with the 3rd 1/4inch metal valves 5,1/2inch stainless steel pipes 10.Pressure vacuum gauge 8 passes through 1/4inch stainless steel tubes
It is connected with one end of the 5th 1/4inch metal valves 9, the other end and the 1/2inch stainless steels of the 5th 1/4inch metal valves 9
Pipeline 10 is weldingly connected, the control of the 5th 1/4inch metal valves 9 and the open and close of pressure vacuum gauge 8.7th 1/4inch metal valves
One end of door 12 is weldingly connected by pipeline and 1/2inch stainless steel pipes 10, the other end of the 7th 1/4inch metal valves 12
It is connected by pipeline with the 6th 1/4inch metal valves 11.One end of 8th 1/4inch metal valves 13 and its exterior
Brominated bromide steel cylinder is connected, and the other end of the 8th 1/4inch metal valves 13 passes through pipeline and the tenth 1/4inch metal valves 16
One end connection, one end that one end of the tenth 1/4inch metal valves 16 passes through pipeline and the 12nd 1/4inch metal valves 19
Connection, the other end and the 1/2inch stainless steel pipes 10 of the 12nd 1/4inch metal valves 19 are weldingly connected；9th 1/4inch
One end of metal valve 14 is connected with the 8th 1/4inch metal valves 13, the tenth 1/4inch metal valves 16 respectively by threeway
Connect, the other end 14 of the 9th 1/4inch metal valves is pushed up by 1/4inch stainless steel tubings and the second brominated bromide holding vessel 15
Portion outlet connection；One end of 11st 1/4inch metal valves 17 by threeway respectively with the tenth 1/4inch metal valves 16,
12nd 1/4inch metal valves 19 connect, and the other end of the 11st 1/4inch metal valves 17 passes through 1/4inch stainless steels
Pipeline is connected with the top exit of tri pentafluorophenyl bromine holding vessel 18.One end of 13rd 1/4inch metal valves 20, the 14th
One end of 4inch metal valves 23 is weldingly connected by pipeline and 1/2inch stainless steel pipes 10；13rd 1/4inch gold
The other end of category valve 20 is connected by pipeline with the entrance of the second metal cold-trap 21, and the outlet of the second metal cold-trap 21 passes through pipe
Line is connected with one end of the first spherical bellows metal valve 22.
Example reaction/separation/purification system includes the 14th 1/4inch metal valves 23, the 3rd metal cold-trap the 24, the tenth
Five 1/4inch metal valves 25, CO2Infrared laser 26, imaging system 27, sample laser cell 28, the second spherical ripple
Pipe metal valve 29, the 4th metal cold-trap 30, the 3rd spherical bellows metal valve 31, fifth metal cold-trap the 32, the 4th are spherical
Bellows metal valve 33, the KBr metals hot trap 34 for filling KBr crystal, the 5th spherical bellows metal valve 35, the 6th metal
36 and the 6th spherical bellows metal valve 37 of cold-trap.One end of 14th 1/4inch metal valves 23 passes through pipeline and 1/
2inch stainless steel pipes 10 are weldingly connected, and the other end of the 14th 1/4inch metal valves 23 is cold by pipeline and the 3rd metal
The entrance connection of trap 24, the outlet of the 3rd metal cold-trap 24 are connected by one end of pipeline and the 15th 1/4inch metal valves 25
Connect, the other end of the 15th 1/4inch metal valves 25 passes through the arrival end of 1/4inch stainless steel tubings and sample laser cell 28
It is weldingly connected, the port of export of sample laser cell 28 passes through 1/4inch stainless steel tubings and the second spherical bellows metal valve 29
One end connection.CO2Infrared laser 26 is to be suspended in the top of sample laser cell 28 not to be joined directly together, imaging system 27 with
CO2Infrared laser 26 integrates, synchronizing moving.The other end of second spherical bellows metal valve 29 by pipeline with
The entrance connection of 4th metal cold-trap 30, the outlet of the 4th metal cold-trap 30 passes through pipeline and the 3rd spherical bellows metal valve
31 one end connection, the other end of the 3rd spherical bellows metal valve 31 pass through pipeline and the arrival end of fifth metal cold-trap 32
Connection, the port of export of fifth metal cold-trap 32 are connected by pipeline with one end of the 4th spherical bellows metal valve 33, and the 4th
The other end of spherical bellows metal valve 33 is connected by pipeline with the entrance for the KBr metals hot trap 34 for filling KBr crystal, is filled
The outlet for filling out the KBr metals hot trap 34 of KBr crystal is connected by pipeline with one end of the 5th spherical bellows metal valve 35, the
The other end of five spherical bellows metal valves 35 is connected by pipeline with the arrival end of the 6th metal cold-trap 36, and the 6th metal is cold
The port of export of trap 36 is connected by pipeline with one end of the 6th spherical bellows metal valve 37.
Collection of products/measurement system includes electric capacity vacuum meter 38, the 7th spherical bellows metal valve 39, the 8th spherical wave
Line pipe metal valve 40,1/2inch stainless steels collecting pipe 41, turbomolecular pump 43, isotope mass spectrometer 44.7th spherical ripple
One end of pipe metal valve 39 is connected by pipeline with the other end of the 6th spherical bellows metal valve 37, the first electric capacity vacuum
Meter 38 is connected with the 6th spherical bellows metal valve 37, the 7th spherical bellows metal valve 39 respectively by threeway；7th
The other end of spherical bellows metal valve 39 by four-way respectively with the 8th spherical bellows metal valve 40, fillingPoint
The double path system sample introduction end connection of the 1/2inch stainless steels collecting pipe 41 and isotope mass spectrometer 44 of son sieve.
Vacuum system includes ion gauge 42 and the turbomolecular pump 43 using rotary vane mechanical pump as prime, turbo-molecular
The inlet end of pump 43 is connected by pipeline with the other end of the first spherical bellows metal valve 22, and ion gauge 42 passes through three
Inlet end, the other end of first spherical bellows metal valve 22 of the reduction of fractions to a common denominator not with turbomolecular pump 43 are connected.
Waste treatment system includes the first 1/4inch metal valves 1, the 2nd 1/4inch metal valves 2, rotary vane type machinery
Vavuum pump 3, the first metal cold-trap 4, the 3rd 1/4inch metal valves 5, the 4th 1/4inch metal valves 6, the first brominated bromide
Holding vessel 7, the 5th 1/4inch metal valves 9,1/2inch stainless steel pipes 10, the 6th 1/4inch metal valves the 11, the 7th 1/
4inch metal valves 12, the 14th 1/4inch metal valves 23, the 3rd metal cold-trap 24 and the 15th 1/4inch metal valves
25.The one end of first 1/4inch metal valves 1 is connected by lateral line with the outlet of the first metal cold-trap 4, the first 1/4inch
The other end of metal valve 1 is connected by pipeline with waste liquid barrel in the fume hood being located at outside the system.2nd 1/4inch metal valves
One end of door 2 is connected by threeway with the lateral line, and the other end of the 2nd 1/4inch metal valves 2 passes through pipeline and blade
The inlet end of formula oil-sealed rotary pump 3 connects.The entrance of first metal cold-trap 4 pass through pipeline and the 3rd 1/4inch metal valves 5 one
End connection, the other end of the 3rd 1/4inch metal valves 5 pass through 1/4inch stainless steel tubings and 1/2inch stainless steel pipes 10
It is weldingly connected；One end of 4th 1/4inch metal valves 6 passes through 1/4inch stainless steel tubings and the first brominated bromide holding vessel 7
Connection, the other ends of the 4th 1/4inch metal valves 6 by threeway respectively with the 3rd 1/4inch metal valves 5,1/2inch not
Rust steel conduit 10 connects.The other end of 5th 1/4inch metal valves 9 is weldingly connected with 1/2inch stainless steel pipes 10.7th
One end of 1/4inch metal valves 12 is weldingly connected by pipeline and 1/2inch stainless steel pipes 10, the 7th 1/4inch metals
The other end of valve 12 is connected by pipeline with one end of the 6th 1/4inch metal valves 11, the 6th 1/4inch metal valves 11
The other end be connected by pipeline with the Ar gas cylinder air outlets outside the system.14th 1/4inch metal valves 23
One end be weldingly connected by pipeline and 1/2inch stainless steel pipes 10, the other end of the 14th 1/4inch metal valves 23 leads to
The entrance that pipeline is crossed with the 3rd metal cold-trap 24 is connected, and the outlet of the 3rd metal cold-trap 24 passes through pipeline and the 15th 1/4inch
One end connection of metal valve 25.
The whole system pipeline and sample laser cell are all designed using 316 type stainless steel materials, and pipeline inwall passes through
Special polishing, the pipeline in addition to metal cold-trap all wind heating tape.
The metal valve is attached by metal ferrule sealing means with pipeline.
It is describedMolecular sieve is filled in external diameter as composition filling in 1/2inch stainless steel tubesThe 1/2inch of molecular sieve is not
Become rusty steel collecting pipe 41, and the 1/2inch stainless steels collecting pipe 41 collects oxygen by liquid nitrogen frozen.
As shown in figure 1, a kind of use above-mentioned high temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system is carried out
High temperature refractory mineral laser-BrF5The method of method oxygen isotope composition analysis, this method specifically comprise the following steps：
Step 1, it is analysed in high temperature refractory mineral samplers loading analysis system
By CO2Infrared laser 26 and imaging system 27 are removed directly over sample laser cell 28, close the analysis
All valves in system, sample laser cell 28 is opened, the high temperature refractory mineral samplers being analysed to load clean sample
In disk and make a record, and the sample disc for filling high temperature refractory mineral samplers to be analyzed is placed in sample laser cell 28, close
Close and tighten sample laser cell 28, complete dress sample operation.
Step 2, a whole set of analysis system is toasted, vacuumizes degassing
Heating charged is opened, with 250 DEG C of carry out heated bakings to the analysis system.Using the heating tape of winding to whole
Individual analysis system carries out heated baking, and baking temperature is 250 DEG C.
The liquid nitrogen cup on the overcoat of the first metal cold-trap 4, slowly open the 15th 1/4inch metal valves 25 and the 14th
4inch metal valves 23, first by the partial air in sample laser cell 28, (" partial air " constitutes about total gas in sample laser cell
/ 5th of body) diffuse in 1/2inch stainless steel tubes main pipeline 10；The 15th 1/4inch metal valves 25 are closed, are opened
3rd 1/4inch metal valves 5 and the 2nd 1/4inch metal valves 2, it is stainless that 1/2inch is taken out by rotary-vane pump 3
Low vacuum (because tolerance is seldom, extracting more than ten seconds, this step operation is not high to vacuum level requirements), closes in steel conduit 10
Close the 14th 1/4inch metal valves 23 and the 3rd 1/4inch metal valves 5.Slowly open the 15th 1/4inch metal valves
25, by the air in sample laser cell 28, (in five times taking most gases in sample laser cell away) is diffused into 1/ by several times
In 2inch stainless steel pipes 10 and low vacuum is taken out by rotary-vane pump 3 (because tolerance is seldom, to extract more than ten seconds
, this step operation is high to vacuum level requirements), it is final to open the 15th 1/4inch metal valves the 25, the 14th completely
4inch metal valves 23, the tenth 1/4inch metal valves 16 and the 12nd 1/4inch metal valves 19.Open the 3rd 1/
Sample low vacuum is to 10 in 4inch metal valves 5 and the sample drawing laser cell 28 of the 2nd 1/4inch metal valves 2-1After Pa20min,
Close the 3rd 1/4inch metal valves 5；The liquid nitrogen cup on the overcoat of the second metal cold-trap 21, open the first spherical bellows metal
Valve 22, the 3rd spherical bellows metal valve 31, the 4th spherical bellows metal valve 33, the 5th spherical bellows metal valve
The 35, the 6th spherical bellows metal valve 37 of door, the 7th spherical 39 and the 8th spherical bellows metal valve of bellows metal valve
Door 40, connection turbomolecular pump 43 is system pumping high vacuum, and by the monitoring system vacuum of ion gauge 42, vacuum reaches
10-6Continue to vacuumize 30min after Pa.
Step 3, to the pre- fluorination treatment of high temperature refractory mineral samplers in sample laser cell 28
After vacuum reaches requirement, heating charged is closed, treats that the analysis system is recovered to room temperature, in the 3rd metal cold-trap 24
With liquid nitrogen cup on the overcoat of the first brominated bromide holding vessel 7；Close the tenth 1/4inch metal valves 16, the 12nd 1/4inch metals
Valve 19, the 14th 1/4inch metal valves 23, the 15th 1/4inch metal valves 25 and the 13rd 1/4inch metal valves
20, after opening the 11st 1/4inch metal valves 17 above tri pentafluorophenyl bromine holding vessel 18, the slow semi-open 12nd
4inch metal valves 19, the BrF diffused in 1/2inch stainless steel tubes main pipeline 10 is controlled by pressure vacuum gauge 85Reagent
Pressure is 0.02MPa, closes the 12nd 1/4inch metal valves 19；Open 1/ after the 14th 1/4inch metal valves 23
BrF in 2inch stainless steel tubes main pipeline 105It is chilled in the 3rd metal cold-trap 24, closes the 14th 1/4inch metal valves
23, the liquid nitrogen cup outside the 3rd metal cold-trap 24 is removed, the naturally to thaw of the 3rd metal cold-trap 24 is recovered to room temperature；Open the 15th
1/4inch metal valves 25, by BrF5After keeping 2min in diffusion of reagents to sample laser cell 28, the 14th is opened successively
4inch metal valves 23, the 4th 1/4inch metal valves 6, by remaining BrF5Reagent is chilled to the first brominated bromide holding vessel 7
It is interior, open the 3rd 1/4inch metal valves 5 and the 2nd 1/4inch metal valves 2, it is impossible to freeze the Residual reactants warp to get off
After crossing the freezing of the first metal cold-trap 4, taken away by rotary-vane pump 3, the closed on the first brominated bromide holding vessel 7
Four 1/4inch metal valves 6.
As stated above in triplicate, fluorination treatment, last time are carried out to sample in sample laser cell 28 and inwall
BrF5Reagent can retain 2h in sample laser cell 28, can remove high temperature refractory mineral samplers and the inwall of sample laser cell 28 completely
The steam of absorption.
Step 4, the high temperature refractory mineral samplers in sample laser cell 28 are carried out with fluorination reaction-O isotopes extraction
After high temperature refractory mineral samplers in sample laser cell 28 complete pre- fluorination treatment, to the analysis system pumping high vacuum
Reach 10-6Continue to take out 30min after Pa, close all valves.The liquid nitrogen cup on the overcoat of the 3rd metal cold-trap 24, open the three or five fluorine
Change the 11st 1/4inch metal valves 17 on bromine holding vessel 18, it is slowly semi-open after opening the 5th 1/4inch metal valves 9
12nd 1/4inch metal valves 19, the BrF repeatedly purified is passed through by the control of pressure vacuum gauge 85Reagent 0.01MPa spreads
To 1/2inch stainless steel tubes main pipeline 10, the 11st 1/4inch metal valves 17 and the 12nd 1/4inch metal valves are closed
Door 19；The 14th 1/4inch metal valves 23 are opened by the BrF in pipeline5Reagent is refrigerated in the 3rd metal cold-trap 24, is closed
14th 1/4inch metal valves 23；Remove the liquid nitrogen cup outside the 3rd metal cold-trap 24 to recover to room temperature, open the 15th
4inch metal valves 25 are by BrF5In diffusion of reagents to sample laser cell 28, the 15th 1/4inch metal valves 25 are closed；Will
CO2Infrared laser 26 is transferred to directly over sample laser cell 28, is positioned by imaging system 27 to high temperature refractory to be analyzed
Directly over mineral samplers, by CO2The laser beam of infrared laser 26 is guided to the sample for filling high temperature refractory mineral samplers to be analyzed
In hole, according to high temperature refractory mineral samplers needs, CO is adjusted2The laser facula size of infrared laser 26 and energy of lasers are right
High temperature refractory mineral samplers to be analyzed carry out heating until " white heat ", high temperature refractory mineral samplers at high temperature with BrF5Reagent enters
Row reaction discharges oxygen, completes the extraction of sample O isotopes.
For example, for olivine particles sample, because it forms temperature height, refractory properties, laser spot diameter can be adjusted
125um is saved, using continuous agitation mode, laser energy is slowly increased to 20W, it is seen that it is existing that " white heat " occurs in olivine mineral
As.
Step 5, O2Purifying, collection and mass spectroscopy
In the 4th metal cold-trap 30, fifth metal cold-trap 32, the 6th metal cold-trap 36 and fillingThe 1/ of molecular sieve
Liquid nitrogen cup on the overcoat of 2inch stainless steels collecting pipe 41, the second spherical bellows metal valve 29 is slowly opened, by laser cell 28
Reactant and remnants BrF5Reagent is chilled in the 4th metal cold-trap 30；The 3rd spherical bellows metal is opened after 10min
Valve 31, by fifth metal cold-trap 32 to reactant and remnants BrF5Reagent freezes again；It is spherical that the 4th is opened after 5min
Bellows metal valve 33, by KBr metals hot trap 34 to reactant and remnants BrF5Reagent further absorbs；Beaten after 5min
The 5th spherical bellows metal valve 35 is opened, the O by the 6th metal cold-trap 36 to generation2Further freezing purifying；After 5min
The 6th spherical bellows metal valve 37 is opened, reaction generation O is monitored by electric capacity vacuum meter 382Pressure；Open the 7th ball
Shape bellows metal valve 39, O2It is collected into and is filled withIn the 1/2inch stainless steels collecting pipe 41 of molecular sieve, pass through electric capacity
Vacuum meter 38 monitors O2Situation about being collected, treats O2The 7th spherical bellows metal valve 39 is closed after being collected completely；Remove and fill
It is filled withLiquid nitrogen outside the 1/2inch stainless steels collecting pipe 41 of molecular sieve, O after recovering to room temperature2It is released, will discharges
O2Introduce isotope mass spectrometer 44 and carry out isotope assay.
Step 6, waste collection processing
, need to be to the remaining BrF that is adsorbed in each cold-trap after completing sample O isotope assays5Reagent and reaction product are carried out
Harmless treatment.
The liquid nitrogen cup on the first metal cold-trap 4, the first brominated bromide holding vessel 7 and the overcoat of the 3rd metal cold-trap 24, close
6th spherical bellows metal valve 37, open the 3rd 1/4inch metal valves 5, the 14th 1/4inch metal valves 23, the
15 1/4inch metal valves 25, the second spherical bellows metal valve 29, the 3rd spherical bellows metal valve the 31, the 4th
Spherical 33 and the 5th spherical bellows metal valve 35 of bellows metal valve, by BrF remaining in system5Reagent and reactant
Pass through the first metal cold-trap 4, the 3rd metal cold-trap 24, the 4th metal cold-trap 30, fifth metal cold-trap 32, the 6th metal cold-trap 36
Carry out after fully freezing；The 2nd 1/4inch metal valves 2 of slow opening are taken away by rotary-vane pump 3 can not be by liquid
The foreign gas of chilled nitrogen, it is spherical to close the 3rd 1/4inch metal valves 5, the 4th spherical bellows metal valve 33 and the 5th
Bellows metal valve 35；It is cold to remove the 3rd metal cold-trap 24, the 4th metal cold-trap 30, the metal of fifth metal cold-trap 32 and the 6th
Liquid nitrogen cup outside trap 36, recovers to room temperature after cold-trap, opens the 4th 1/4inch metal valves 6 by the first metal cold-trap 4, the
Three metal cold-traps 24, the 4th metal cold-trap 30, fifth metal cold-trap 32, the remaining BrF of 36 interior freezing of the 6th metal cold-trap5Reagent
And reaction product is refrigerated in the first brominated bromide holding vessel 7；The 4th 1/4inch metal valves 6 are closed, open the 3rd 1/
4inch metal valves 5, the 4th spherical 33 and the 5th spherical bellows metal valve 35 of bellows metal valve, pass through rotary vane type
Oil-sealed rotary pump 3 further takes out low vacuum to systematic pipeline to 10-1Pa, possible remaining impurity in the analysis system is frozen in
In first metal cold-trap 4；All valves are closed, remove the liquid nitrogen cup outside the first metal cold-trap 4, open the 6th 1/4inch successively
Metal valve 11, the 7th 1/4inch metal valves 12, the 3rd 1/4inch metal valves 5 and the first 1/4inch metal valves 1,
The Litter that will likely be remained is downloaded in the lime bucket in fume hood with Ar fates, completes Waste disposal, avoids polluting environment.
The present invention is explained in detail above in conjunction with drawings and examples, but the present invention is not limited to above-mentioned implementation
Example, in those of ordinary skill in the art's possessed knowledge, can also make on the premise of present inventive concept is not departed from
Go out various change.The content not being described in detail in the present invention can use prior art.
Claims (23)
- A kind of 1. high temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system, it is characterised in that：The system includes examination Agent purification system, example reaction/separation/purification system, collection of products/measurement system and vacuum system；Reagent purification system point One end not with example reaction/separate/purification system, vacuum system connects, example reaction/separation/purification system other end with One end connection of collection of products/measurement system, the other end of collection of products/measurement system are connected with vacuum system.
- A kind of 2. high temperature refractory mineral laser-BrF according to claim 15Method oxygen isotope composition analysis system, it is special Sign is：Described reagent purification system includes rotary-vane pump (3), the first metal cold-trap (4), the first brominated bromide Holding vessel (7), pressure vacuum gauge (8), 1/2inch stainless steel pipes (10), the second brominated bromide holding vessel (15), the three or five fluorine Change bromine holding vessel (18), the second metal cold-trap (21), the top of 1/2inch stainless steel pipes (10) is provided with pressure vacuum gauge (8), the side top of 1/2inch stainless steel pipes (10) respectively with first brominated bromide holding vessel (7) top exit, the first gold medal Belong to the connection of cold-trap (4) entrance, the outlet of the first metal cold-trap (4) is connected with rotary-vane pump (3) inlet end；1/2inch One side bottom of stainless steel pipes (10) pushes up with the second brominated bromide holding vessel (15), tri pentafluorophenyl bromine holding vessel (18) respectively Portion outlet connection, another upper lateral part of 1/2inch stainless steel pipes (10) are connected with second metal cold-trap (21) entrance.
- A kind of 3. high temperature refractory mineral laser-BrF according to claim 25Method oxygen isotope composition analysis system, it is special Sign is：The 5th 1/4inch gold is provided between the top of described 1/2inch stainless steel pipes (10) and pressure vacuum gauge (8) Belong to valve (9).
- A kind of 4. high temperature refractory mineral laser-BrF according to claim 35Method oxygen isotope composition analysis system, it is special Sign is：The 4th 1/4inch is provided between described 1/2inch stainless steel pipes (10) and the first brominated bromide holding vessel (7) Metal valve (6), the 3rd 1/4inch metals are provided between 1/2inch stainless steel pipes (10) and first metal cold-trap (4) entrance Valve (5), the 2nd 1/4inch metals are provided between the outlet of the first metal cold-trap (4) and rotary-vane pump (3) inlet end Valve (2), first metal cold-trap (4) exit are additionally provided with first 1/4inch in parallel with the 2nd 1/4inch metal valves (2) Metal valve (1).
- A kind of 5. high temperature refractory mineral laser-BrF according to claim 45Method oxygen isotope composition analysis system, it is special Sign is：Set between described 1/2inch stainless steel pipes (10) bottom and tri pentafluorophenyl bromine holding vessel (18) top exit There are the 12nd 1/4inch metal valves (19), the 11st 1/4inch metal valves (17), the 12nd 1/4inch metal valves (19) the 10th, is provided between the 11st 1/4inch metal valves (17) and second brominated bromide holding vessel (15) top exit 4inch metal valves (16), the 9th 1/4inch metal valves (14), the tenth 1/4inch metal valves (16) and the 9th 1/ The 8th 1/4inch metal valves (13) being all connected with both are provided between 4inch metal valves (14).
- A kind of 6. high temperature refractory mineral laser-BrF according to claim 55Method oxygen isotope composition analysis system, it is special Sign is：One middle side part of described 1/2inch stainless steel pipes (10) also connects with the 7th 1/4inch metal valves (12) one end Connect, the 7th 1/4inch metal valves (12) other end is connected with the 6th 1/4inch metal valves (11).
- A kind of 7. high temperature refractory mineral laser-BrF according to claim 65Method oxygen isotope composition analysis system, it is special Sign is：The tenth is provided between the opposite side of described 1/2inch stainless steel pipes (10) and second metal cold-trap (21) entrance Three 1/4inch metal valves (20) connect, and second metal cold-trap (21) exit is provided with the first spherical bellows metal valve (22), the first spherical bellows metal valve (22) is connected with vacuum system.
- A kind of 8. high temperature refractory mineral laser-BrF according to claim 75Method oxygen isotope composition analysis system, it is special Sign is：Described example reaction/separation/purification system includes the 3rd metal cold-trap (24), CO2Infrared laser (26), into As observing system (27), sample laser cell (28), the 4th metal cold-trap (30), fifth metal cold-trap (32), KBr metal hot traps (34) and the 6th metal cold-trap (36), the 3rd metal cold-trap (24) entrance and the 13rd 1/4inch metals of reagent purification system Valve (20) is connected, and the outlet of the 3rd metal cold-trap (24) is connected with one end of sample laser cell (28), sample laser cell (28) The other end is connected with the arrival end of the 4th metal cold-trap (30), the port of export and the fifth metal cold-trap of the 4th metal cold-trap (30) (32) arrival end connection, the port of export of fifth metal cold-trap (32) are connected with the arrival end of KBr metals hot trap (34), KBr gold The port of export of category hot trap (34) is connected with the arrival end of the 6th metal cold-trap (36), the port of export of the 6th metal cold-trap (36) and production Thing collection/measurement system connection；Sample laser cell (28) is provided with CO2Infrared laser (26), CO2On infrared laser (26) Provided with imaging system (27).
- A kind of 9. high temperature refractory mineral laser-BrF according to claim 85Method oxygen isotope composition analysis system, it is special Sign is：The 14th 1/4inch is provided between the 3rd described metal cold-trap (24) entrance and 1/2inch stainless steel pipes (10) Metal valve (23), the 15th 1/4inch metal valves are provided between the outlet of the 3rd metal cold-trap (24) and sample laser cell (28) Door (25), is provided with the second spherical bellows metal valve (29) between sample laser cell (28) and the 4th metal cold-trap (30), the Three spherical bellows metal valves (31), fifth metal cold-trap are provided between four metal cold-traps (30) and fifth metal cold-trap (32) (32) the 4th spherical bellows metal valve (33), KBr metals hot trap (34) and the 6th are provided between KBr metals hot trap (34) The 5th spherical bellows metal valve (35), the 6th metal cold-trap (36) and collection of products/survey are provided between metal cold-trap (36) Determine to be provided with the 6th spherical bellows metal valve (37) between system.
- A kind of 10. high temperature refractory mineral laser-BrF according to claim 95Method oxygen isotope composition analysis system, it is special Sign is：Described collection of products/measurement system include electric capacity vacuum meter (38), the 7th spherical bellows metal valve (39), 8th spherical bellows metal valve (40), 1/2inch stainless steels collecting pipe (41), turbomolecular pump (43), isotope mass spectrometry Instrument (44), one end of the 7th spherical bellows metal valve (39) pass through the 6th of pipeline and example reaction/separate/purification system The connection of spherical bellows metal valve (37), electric capacity vacuum meter (38) respectively with the 6th spherical bellows metal valve (37), the Seven spherical bellows metal valve (39) connections；The other end of 7th spherical bellows metal valve (39) is spherical with the 8th respectively Bellows metal valve (40), 1/2inch stainless steels collecting pipe (41) and isotope mass spectrometer (44) connection.
- A kind of 11. high temperature refractory mineral laser-BrF according to claim 105Method oxygen isotope composition analysis system, its It is characterised by：Described vacuum system includes ion gauge (42) and the turbomolecular pump using rotary vane mechanical pump as prime (43), turbomolecular pump (43) is connected with the first spherical bellows metal valve (22) of reagent purification system, ion gauge (42) it is connected respectively with turbomolecular pump (43), the first spherical bellows metal valve (22).
- A kind of 12. high temperature refractory mineral laser-BrF according to claim 115Method oxygen isotope composition analysis system, its It is characterised by：Described analysis system also includes waste treatment system, and waste treatment system includes the first 1/4inch metal valves (1), the 2nd 1/4inch metal valves (2), rotary-vane pump (3), the first metal cold-trap (4), the 3rd 1/4inch gold Belong to valve (5), the 4th 1/4inch metal valves (6), the first brominated bromide holding vessel (7), the 5th 1/4inch metal valves (9), 1/2inch stainless steel pipes (10), the 6th 1/4inch metal valves (11), the 7th 1/4inch metal valves (12), 14 1/4inch metal valves (23), the 3rd metal cold-trap (24) and the 15th 1/4inch metal valves (25), the one 1/ 4inch metal valves (1) one end is connected with the outlet of the first metal cold-trap (4), one end of the 2nd 1/4inch metal valves (2) Outlet with the first 1/4inch metal valves (1), the first metal cold-trap (4) is connected, the 2nd 1/4inch metal valves (2) it is another One end is connected with rotary-vane pump (3) inlet end；The entrance and the 3rd 1/4inch metal valves of first metal cold-trap (4) One end connection of door (5), the other end of the 3rd 1/4inch metal valves (5) are connected with 1/2inch stainless steel pipes (10)；The One end of four 1/4inch metal valves (6) is connected with the first brominated bromide holding vessel (7), the 4th 1/4inch metal valves (6) The other end be connected respectively with the 3rd 1/4inch metal valves (5), 1/2inch stainless steel pipes (10)；5th 1/4inch gold The other end of category valve (9) is connected with 1/2inch stainless steel pipes (10)；One end of 7th 1/4inch metal valves (12) with 1/2inch stainless steel pipes (10) connect, the other end and the 6th 1/4inch metal valves of the 7th 1/4inch metal valves (12) One end connection of door (11)；One end of 14th 1/4inch metal valves (23) is connected with 1/2inch stainless steel pipes (10), The other end of 14th 1/4inch metal valves (23) is connected with the entrance of the 3rd metal cold-trap (24), the 3rd metal cold-trap (24) outlet is connected with one end of the 15th 1/4inch metal valves (25).
- A kind of 13. high temperature refractory mineral laser-BrF using described in the claims 1 to 125Method oxygen isotope composition analysis System carries out high temperature refractory mineral laser-BrF5The method of method oxygen isotope composition analysis, it is characterised in that this method is specifically wrapped Include following steps：Step 1, it is analysed in high temperature refractory mineral samplers loading analysis system；Step 2, a whole set of analysis system is toasted, vacuumizes degassing；Step 3, to the pre- fluorination treatment of high temperature refractory mineral samplers in sample laser cell；Step 4, the high temperature refractory mineral samplers in sample laser cell are carried out with fluorination reaction-O isotopes extraction；Step 5, O2Purifying, collection and mass spectroscopy；Step 6, waste collection processing.
- 14. high temperature refractory mineral laser-BrF according to claim 135The method of method oxygen isotope composition analysis, it is special Sign is that described step 1 comprises the following steps that：By CO2Infrared laser (26) and imaging system (27) are removed directly over sample laser cell (28), close the analysis All valves in system, sample laser cell (28) is opened, the high temperature refractory mineral samplers being analysed to load clean sample In product disk and make a record, and the sample disc for filling high temperature refractory mineral samplers to be analyzed is placed on sample laser cell (28) It is interior, close and tighten sample laser cell (28), complete dress sample operation.
- 15. high temperature refractory mineral laser-BrF according to claim 145The method of method oxygen isotope composition analysis, it is special Sign is that described step 2 comprises the following steps that：Heating charged is opened, heated baking is carried out to the analysis system；The liquid nitrogen cup on first metal cold-trap (4) overcoat, beats The 15th 1/4inch metal valves (25) and the 14th 1/4inch metal valves (23) are opened, first by sample laser cell (28) Partial air is diffused in 1/2inch stainless steel tubes main pipeline (10)；The 15th 1/4inch metal valves (25) are closed, are opened 3rd 1/4inch metal valves (5) and the 2nd 1/4inch metal valves (2), 1/ is taken out by rotary-vane pump (3) 2inch stainless steel pipes (10) interior low vacuum, close the 14th 1/4inch metal valves (23) and the 3rd 1/4inch metal valves Door (5).The 15th 1/4inch metal valves (25) are slowly opened, the air in sample laser cell (28) is diffused into 1/ by several times Low vacuum is taken out in 2inch stainless steel pipes (10) and by rotary-vane pump (3), it is final to open the 15th completely 4inch metal valves (25), the 14th 1/4inch metal valves (23), the tenth 1/4inch metal valves (16) and the 12nd 4inch metal valves (19)；Open the 3rd 1/4inch metal valves (5) and the 2nd 1/4inch metal valves (2) sample drawing swashs In light pond (28) after sample low vacuum 20min, the 3rd 1/4inch metal valves (5) are closed；In second metal cold-trap (21) overcoat Upper liquid nitrogen cup, open the first spherical bellows metal valve (22), the 3rd spherical bellows metal valve (31), the 4th spherical wave Line pipe metal valve (33), the 5th spherical bellows metal valve (35), the 6th spherical bellows metal valve (37), the 7th ball Shape bellows metal valve (39) and the 8th spherical bellows metal valve (40), connection turbomolecular pump (43) are that system takes out height Continue to vacuumize 30min after vacuum, pass through ion gauge (42) monitoring system vacuum.
- 16. high temperature refractory mineral laser-BrF according to claim 155The method of method oxygen isotope composition analysis, it is special Sign is：System heated baking temperature in described step 2 is 250 DEG C；Turbomolecular pump (43) be system pumping high vacuum extremely Vacuum is 10-6Pa。
- 17. high temperature refractory mineral laser-BrF according to claim 165The method of method oxygen isotope composition analysis, it is special Sign is that described step 3 comprises the following steps that：Heating charged is closed, treats that the analysis system is recovered to room temperature, is stored up in the 3rd metal cold-trap (24) and the first brominated bromide Deposit liquid nitrogen cup on tank (7) overcoat；Close the tenth 1/4inch metal valves (16), the 12nd 1/4inch metal valves (19), 14 1/4inch metal valves (23), the 15th 1/4inch metal valves (25) and the 13rd 1/4inch metal valves (20), After opening the 11st 1/4inch metal valves (17) above tri pentafluorophenyl bromine holding vessel (18), the slow semi-open 12nd 1/4inch metal valves (19), diffused to by pressure vacuum gauge (8) control in 1/2inch stainless steel tubes main pipeline (10) BrF5Reagent pressure, close the 12nd 1/4inch metal valves (19)；Open the 14th 1/4inch metal valves (23) afterwards 1/ BrF in 2inch stainless steel tubes main pipeline (10)5It is chilled in the 3rd metal cold-trap (24), closes the 14th 1/4inch metals Valve (23), removes the liquid nitrogen cup of the 3rd metal cold-trap (24) outside, and the 3rd metal cold-trap (24) naturally to thaw is recovered to room temperature； The 15th 1/4inch metal valves (25) are opened, by BrF5After keeping 2min in diffusion of reagents to sample laser cell (28), successively The 14th 1/4inch metal valves (23), the 4th 1/4inch metal valves (6) are opened, by remaining BrF5Reagent is chilled to first In brominated bromide holding vessel (7), the 3rd 1/4inch metal valves (5) and the 2nd 1/4inch metal valves (2) are opened, it is impossible to cold The Residual reactants frozen are taken away after the freezing of the first metal cold-trap (4) by rotary-vane pump (3), close The 4th 1/4inch metal valves (6) on first brominated bromide holding vessel (7).
- 18. high temperature refractory mineral laser-BrF according to claim 175The method of method oxygen isotope composition analysis, it is special Sign is：The BrF that pressure vacuum gauge (8) control is diffused in 1/2inch stainless steel tubes main pipeline (10) in described step 35 Reagent pressure is 0.02MPa.
- 19. high temperature refractory mineral laser-BrF according to claim 185The method of method oxygen isotope composition analysis, it is special Sign is：By above-mentioned steps 3 method in triplicate, fluorination treatment is carried out to the interior sample of sample laser cell (28) and inwall, most A BrF afterwards5Reagent retains 2h in sample laser cell (28), removes high temperature refractory mineral samplers and sample laser cell completely (28) steam of inwall absorption.
- 20. high temperature refractory mineral laser-BrF according to claim 195The method of method oxygen isotope composition analysis, it is special Sign is that described step 4 comprises the following steps that：After high temperature refractory mineral samplers in sample laser cell (28) complete pre- fluorination treatment, the analysis system pumping high vacuum is reached To 10-6Continue to take out 30min after Pa, close all valves；The liquid nitrogen cup on the 3rd metal cold-trap (24) overcoat, open the three or five fluorine Change the 11st 1/4inch metal valves (17) on bromine holding vessel (18), after opening the 5th 1/4inch metal valves (9), slowly Semi-open 12nd 1/4inch metal valves (19), the BrF repeatedly purified is passed through by pressure vacuum gauge (8) control5Reagent 0.01MPa is diffused in 1/2inch stainless steel tubes main pipeline (10), closes the 11st 1/4inch metal valves (17) and the tenth Two 1/4inch metal valves (19)；The 14th 1/4inch metal valves (23) are opened by the BrF in pipeline5Reagent is refrigerated to In three metal cold-traps (24), the 14th 1/4inch metal valves (23) are closed；Remove the liquid nitrogen cup of the 3rd metal cold-trap (24) outside Recover to room temperature, open the 15th 1/4inch metal valves (25) by BrF5In diffusion of reagents to sample laser cell (28), close 15th 1/4inch metal valves (25)；By CO2Infrared laser (26) is transferred to directly over sample laser cell (28), is passed through into Directly over observing system (27) positioning to high temperature refractory mineral samplers to be analyzed, by CO2The laser beam of infrared laser (26) In guiding to the sample well for filling high temperature refractory mineral samplers to be analyzed, CO is adjusted2The laser facula size of infrared laser (26) And energy of lasers, high temperature refractory mineral samplers to be analyzed are heated, high temperature refractory mineral samplers at high temperature with BrF5 Reagent carries out reaction and discharges oxygen, completes the extraction of sample O isotopes.
- 21. high temperature refractory mineral laser-BrF according to claim 205The method of method oxygen isotope composition analysis, it is special Sign is that described step 5 comprises the following steps that：In the 4th metal cold-trap (30), fifth metal cold-trap (32), the 6th metal cold-trap (36) and 1/2inch stainless steel collecting pipes (41) liquid nitrogen cup on overcoat, slowly open the second spherical bellows metal valve (29), by the reactant in laser cell (28) and Remaining BrF5Reagent is chilled in the 4th metal cold-trap (30)；The 3rd spherical bellows metal valve (31) is opened after 10min, By fifth metal cold-trap (32) to reactant and remnants BrF5Reagent freezes again；The 4th spherical bellows is opened after 5min Metal valve (33), by KBr metals hot trap (34) to reactant and remnants BrF5Reagent further absorbs；Opened after 5min 5th spherical bellows metal valve (35), the O by the 6th metal cold-trap (36) to generation2Further freezing purifying；5min The 6th spherical bellows metal valve (37) is opened afterwards, and reaction generation O is monitored by electric capacity vacuum meter (38)2Pressure；Open 7th spherical bellows metal valve (39), O2It is collected into fillingIn the 1/2inch stainless steels collecting pipe (41) of molecular sieve, O is monitored by electric capacity vacuum meter (38)2Situation about being collected, treats O2The 7th spherical bellows metal valve is closed after being collected completely Door (39)；Remove the liquid nitrogen of 1/2inch stainless steels collecting pipe (41) outside, O after recovering to room temperature2It is released, will discharges O2Introduce isotope mass spectrometer (44) and carry out isotope assay.
- 22. high temperature refractory mineral laser-BrF according to claim 215The method of method oxygen isotope composition analysis, it is special Sign is：It is filled with 1/2inch stainless steels collecting pipe (41) in described step 5Molecular sieve.
- 23. high temperature refractory mineral laser-BrF according to claim 225The method of method oxygen isotope composition analysis, it is special Sign is：Described step 6 comprises the following steps that：The liquid nitrogen cup on the first metal cold-trap (4), the first brominated bromide holding vessel (7) and the 3rd metal cold-trap (24) overcoat, close The 6th spherical bellows metal valve (37) is closed, opens the 3rd 1/4inch metal valves (5), the 14th 1/4inch metal valves (23), the 15th 1/4inch metal valves (25), the second spherical bellows metal valve (29), the 3rd spherical bellows metal Valve (31), the 4th spherical bellows metal valve (33) and the 5th spherical bellows metal valve (35), will be remaining in system BrF5Reagent and reactant pass through the first metal cold-trap (4), the 3rd metal cold-trap (24), the 4th metal cold-trap (30), the 5th Metal cold-trap (32), the 6th metal cold-trap (36) are carried out after fully freezing；It is logical slowly to open the 2nd 1/4inch metal valves (2) Cross rotary-vane pump (3) take away can not by the foreign gas of liquid nitrogen frozen, close the 3rd 1/4inch metal valves (5), 4th spherical bellows metal valve (33) and the 5th spherical bellows metal valve (35)；Remove the 3rd metal cold-trap (24), 4th metal cold-trap (30), the liquid nitrogen cup of fifth metal cold-trap (32) and the 6th metal cold-trap (36) outside, treat that cold-trap recovers to room Wen Hou, open the 4th 1/4inch metal valves (6) the first metal cold-trap (4), the 3rd metal cold-trap (24), the 4th metal is cold The remaining BrF of freezing in trap (30), fifth metal cold-trap (32), the 6th metal cold-trap (36)5Reagent and reaction product are refrigerated to In first brominated bromide holding vessel (7)；The 4th 1/4inch metal valves (6) are closed, open the 3rd 1/4inch metal valves (5), the 4th spherical bellows metal valve (33) and the 5th spherical bellows metal valve (35), pass through rotary vane type mechanical vacuum Pump (3) further takes out low vacuum to systematic pipeline, and impurity remaining in the analysis system is frozen in into the first metal cold-trap (4) It is interior；All valves are closed, remove the liquid nitrogen cup of the first metal cold-trap (4) outside, open the 6th 1/4inch metal valves successively (11), the 7th 1/4inch metal valves (12), the 3rd 1/4inch metal valves (5) and the first 1/4inch metal valves (1), The Litter of residual is downloaded in the lime bucket in fume hood with Ar fates, completes Waste disposal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710656902.4A CN107402252B (en) | 2017-08-03 | 2017-08-03 | High temperature refractory mineral laser-BrF 5 System and method for analyzing oxygen isotope composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710656902.4A CN107402252B (en) | 2017-08-03 | 2017-08-03 | High temperature refractory mineral laser-BrF 5 System and method for analyzing oxygen isotope composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107402252A true CN107402252A (en) | 2017-11-28 |
| CN107402252B CN107402252B (en) | 2024-03-22 |
Family
ID=60401391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710656902.4A Active CN107402252B (en) | 2017-08-03 | 2017-08-03 | High temperature refractory mineral laser-BrF 5 System and method for analyzing oxygen isotope composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107402252B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109596701A (en) * | 2019-01-17 | 2019-04-09 | 中国地质科学院矿产资源研究所 | Method and device for analyzing silicon isotope composition |
| CN110887721A (en) * | 2018-09-07 | 2020-03-17 | 核工业理化工程研究院 | Sample purification device and sample purification method for gas isotope analysis |
| CN115060783A (en) * | 2022-08-16 | 2022-09-16 | 中国科学院地质与地球物理研究所 | Carbonate total oxygen isotope measuring system and measuring method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2124621A1 (en) * | 1971-02-10 | 1972-09-22 | American Cyanamid Co | Ammonation and hydration of chloro ,and fluoro - cpds - induced by infra red laser |
| SU972312A1 (en) * | 1980-09-16 | 1982-11-07 | Институт Литосферы Ан Ссср | Method of extracting oxygen from minerals for isotope analysis |
| US5666639A (en) * | 1994-06-07 | 1997-09-09 | Iti Group Llc | CRISLA process and apparatus |
| JP2005083839A (en) * | 2003-09-05 | 2005-03-31 | Japan Science & Technology Agency | Method of measuring ratio of three kinds of stable oxygen isotopes in atmosphere or dissolved gas, and o2 isolation device used therefor |
| US20080028830A1 (en) * | 2003-12-19 | 2008-02-07 | Wei Li | Method and System to Separate and Measure 37Ar Quickly |
| CN101799450A (en) * | 2010-03-22 | 2010-08-11 | 上海华质生物技术有限公司 | Device and method for detecting volatile organic compound |
| CN102012333A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Device for purifying and enriching inert gases and use method |
| CN102338711A (en) * | 2010-07-22 | 2012-02-01 | 中国石油天然气股份有限公司 | Sample preparation system with functions of extraction and separation of inert gas, and use thereof |
| CN204389453U (en) * | 2014-12-31 | 2015-06-10 | 中国地质科学院矿产资源研究所 | Nitrogen oxygen isotope measuring device of trace nitrate sample |
| CN206177666U (en) * | 2016-10-31 | 2017-05-17 | 核工业北京地质研究院 | A draw purification system for xenon is dissolved to aquatic |
| CN207457129U (en) * | 2017-08-03 | 2018-06-05 | 核工业北京地质研究院 | High temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system |
-
2017
- 2017-08-03 CN CN201710656902.4A patent/CN107402252B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2124621A1 (en) * | 1971-02-10 | 1972-09-22 | American Cyanamid Co | Ammonation and hydration of chloro ,and fluoro - cpds - induced by infra red laser |
| SU972312A1 (en) * | 1980-09-16 | 1982-11-07 | Институт Литосферы Ан Ссср | Method of extracting oxygen from minerals for isotope analysis |
| US5666639A (en) * | 1994-06-07 | 1997-09-09 | Iti Group Llc | CRISLA process and apparatus |
| JP2005083839A (en) * | 2003-09-05 | 2005-03-31 | Japan Science & Technology Agency | Method of measuring ratio of three kinds of stable oxygen isotopes in atmosphere or dissolved gas, and o2 isolation device used therefor |
| US20080028830A1 (en) * | 2003-12-19 | 2008-02-07 | Wei Li | Method and System to Separate and Measure 37Ar Quickly |
| CN102012333A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Device for purifying and enriching inert gases and use method |
| CN101799450A (en) * | 2010-03-22 | 2010-08-11 | 上海华质生物技术有限公司 | Device and method for detecting volatile organic compound |
| CN102338711A (en) * | 2010-07-22 | 2012-02-01 | 中国石油天然气股份有限公司 | Sample preparation system with functions of extraction and separation of inert gas, and use thereof |
| CN204389453U (en) * | 2014-12-31 | 2015-06-10 | 中国地质科学院矿产资源研究所 | Nitrogen oxygen isotope measuring device of trace nitrate sample |
| CN206177666U (en) * | 2016-10-31 | 2017-05-17 | 核工业北京地质研究院 | A draw purification system for xenon is dissolved to aquatic |
| CN207457129U (en) * | 2017-08-03 | 2018-06-05 | 核工业北京地质研究院 | High temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system |
Non-Patent Citations (3)
| Title |
|---|
| 万德芳 等: "硫酸盐的氧同位素测量方法", vol. 12, no. 3, pages 378 - 383 * |
| 李铁军: "氧同位素在岩石成因研究的新进展", vol. 32, no. 6, pages 841 - 849 * |
| 龚冰 等: "硅酸盐和金属氧化物矿物氧同位素组成的CO2激光氟化分析", vol. 20, no. 4, pages 428 - 430 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887721A (en) * | 2018-09-07 | 2020-03-17 | 核工业理化工程研究院 | Sample purification device and sample purification method for gas isotope analysis |
| CN109596701A (en) * | 2019-01-17 | 2019-04-09 | 中国地质科学院矿产资源研究所 | Method and device for analyzing silicon isotope composition |
| CN115060783A (en) * | 2022-08-16 | 2022-09-16 | 中国科学院地质与地球物理研究所 | Carbonate total oxygen isotope measuring system and measuring method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107402252B (en) | 2024-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107422024A (en) | The analysis system and method for not oxygen-containing mineral inclusion water oxygen isotopics | |
| CN107402252A (en) | High temperature refractory mineral laser BrF5Method oxygen isotope composition analysis system and method | |
| CN207457129U (en) | High temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system | |
| CN105513654B (en) | Multiple spot quickly surveys the device and its implementation of hydrogen after nuclear power plant containment shell accident | |
| CN104048860B (en) | Sample preparation device and sample preparation method for sulfur isotope analysis | |
| CN105369041A (en) | Sodium-potassium alloy vacuum distillation device | |
| CN105233629B (en) | A kind of gas absorbing device and technique | |
| CN207379974U (en) | The analysis system of not oxygen-containing mineral inclusion water oxygen isotopics | |
| CN201470295U (en) | Collecting device of carbon dioxide generated by carbonate and phosphoric acid | |
| CN205205205U (en) | Na -K alloy vacuum distillation plant | |
| CN106568614A (en) | A sampling device for dissolved gas analysis of a water sample and a sampling method thereof | |
| CN110031536A (en) | Oxygen isotope composition analysis extraction element and method in a kind of rock and mineral | |
| CN106644618B (en) | Gas sampling system and application thereof | |
| CN108303297B (en) | Dual-purpose hydrogen method and zinc method 14 C sample preparation system | |
| CN211318298U (en) | Oxygen isotope composition analysis extraction element in rock and mineral | |
| JP2734722B2 (en) | Geothermal well two-phase fluid separation and sampling device | |
| CN206177666U (en) | A draw purification system for xenon is dissolved to aquatic | |
| CN111128428A (en) | Tritium tail gas rapid collecting and processing device | |
| CN207946261U (en) | A kind of hydrogen method and zinc method are dual-purpose14C sample preparation system | |
| CN111693652B (en) | Analysis method and treatment system for chlorine-containing waste gas generated by high-temperature water quenching of chlorination slag | |
| CN208872701U (en) | Carbon and hydrogen isotope analysis system for mineral fluid inclusion | |
| CN206177636U (en) | Sampling device of water sample dissolved gas analysis | |
| CN115200962B (en) | Graphite sample preparation system and sample preparation method for accelerator mass spectrum | |
| CN207556918U (en) | A kind of hydrofluoric acid sampler | |
| CN219377070U (en) | Pyrolysis experiment product collecting system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |